HPLC同时测定川芎、当归SFE-CO萃取物中7种成分含量及阿魏酸松柏酯稳定性考察

马云桐; 徐世军; 廖海浪; 何芳; 钟芙蓉; 文雯; 吴督督

doi:10.13422/j.cnki.syfjx.2017090024

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HPLC同时测定川芎、当归SFE-CO萃取物中7种成分含量及阿魏酸松柏酯稳定性考察

化学与分析 | 更新时间：2024-01-04

- HPLC同时测定川芎、当归SFE-CO萃取物中7种成分含量及阿魏酸松柏酯稳定性考察
- HPLC Simultaneous Determination of Seven Components in SFE-CO Extract from Chuanxiong Rhizoma and Angelicae Sinensis Radix and Stability Investigation of Coniferyl Ferulate
- 中国实验方剂学杂志 2017年23卷第9期页码：24-29
- 作者机构：
- 作者简介：
- 基金信息：
  
  国家“重大新药创制”科技重大专项（2013ZX09103002-008）;国家基础科学人才培养基金项目（J13100340-20）;四川省科技计划（2013SZ0131）
- DOI：10.13422/j.cnki.syfjx.2017090024
  中图分类号： O657.72;R284.1
- 纸质出版日期：2017
- 稿件说明：
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马云桐, 徐世军, 廖海浪, 等. HPLC同时测定川芎、当归SFE-CO萃取物中7种成分含量及阿魏酸松柏酯稳定性考察[J]. 中国实验方剂学杂志, 2017,23(9):24-29.

MA Yun-tong, XU Shi-jun, LIAO Hai-lang, et al. HPLC Simultaneous Determination of Seven Components in SFE-CO Extract from Chuanxiong Rhizoma and Angelicae Sinensis Radix and Stability Investigation of Coniferyl Ferulate[J]. Chinese journal of experimental traditional medical formulae, 2017, 23(9): 24-29.
马云桐, 徐世军, 廖海浪, 等. HPLC同时测定川芎、当归SFE-CO萃取物中7种成分含量及阿魏酸松柏酯稳定性考察[J]. 中国实验方剂学杂志, 2017,23(9):24-29. DOI： 10.13422/j.cnki.syfjx.2017090024.

MA Yun-tong, XU Shi-jun, LIAO Hai-lang, et al. HPLC Simultaneous Determination of Seven Components in SFE-CO Extract from Chuanxiong Rhizoma and Angelicae Sinensis Radix and Stability Investigation of Coniferyl Ferulate[J]. Chinese journal of experimental traditional medical formulae, 2017, 23(9): 24-29. DOI： 10.13422/j.cnki.syfjx.2017090024.

摘要

目的：建立HPLC法同步测定川芎、当归SFE-CO2萃取物中7种成分含量的方法，并考察其中阿魏酸松柏酯的稳定性。方法：以二氯甲烷为助溶剂，甲醇、乙腈和5%甲酸甲醇为溶剂，考察2种萃取物中阿魏酸松柏酯稳定性。HPLC分析采用Wondasil C18-WR色谱柱（4.6 mm×250 mm，5 μm），以乙腈-0.5%乙酸水为流动相梯度洗脱，流速1.0 mL·min-1，柱温35℃，检测波长270 nm，测定2种萃取物中7种成分含量。结果：乙腈溶液中，2种萃取物中阿魏酸松柏酯稳定性均最佳。经测定2种萃取物均含有阿魏酸，洋川芎内酯I，洋川芎内酯H，阿魏酸松柏酯，洋川芎内酯A，藁本内酯和丁烯基苯酞7种物质，其线性关系、精密度、重复性、稳定性、加样回收率均良好。对于川芎SFE-CO2萃取物，它们的线性范围分别在2.41~24.14，3.83~38.26，0.81~8.08，47.43~474.32，95.49~954.91，164.91~1 649.14，3.32~33.24 ng；平均加样回收率分别为95.04%，98.24%，99.03%，98.46%，98.13%，96.97%，95.20%，RSD分别为2.9%，1.2%，1.6%，1.2%，1.1%，1.4%，1.2%。对于当归SFE-CO2萃取物，它们的线性范围分别在1.31~13.15，1.70~17.01，0.44~4.43，27.52~275.18，6.46~64.60，206.19~2 061.92，3.07~30.65 ng；平均加样回收率分别为99.03%，99.00%，103.15%，101.78%，102.12%，100.01%，102.49%，RSD分别为2.1%，2.2%，2.2%，2.1%，2.1%，2.5%，2.2%。结论：阿魏酸松柏酯易分解成阿魏酸，选乙腈溶解可保证原阿魏酸及阿魏酸松柏酯含量准确测定，该含量方法简单、快速，可为川芎、当归SFE-CO2萃取物的质量标准提供依据。

Abstract

Objective: To establish an HPLC method for simultaneously determining seven components in SFE-CO2 extract of Chuanxiong Rhizoma and Angelicae Sinensis Radix

and investigate the stability of coniferyl ferulate. Method: The stability of coniferyl ferulate was evaluated with CH2Cl2 as the cosolvent

and methanol

acetonitrile or 5% formic acid in methanol as the solvent. The HPLC method was performed on wondasil C18-WR column (4.6 mm×250 mm

5 μm) with acetonitrile-0.3% acetic acid solution as mobile phase for gradient elution; the flow rate was 1.0 mL·min-1; column temperature was 35℃

and the detection wavelength was 270 nm. Result: The stability of coniferyl ferulate in the two SFE-CO2 extracts was best with the acetonitrile as solven. The seven components (ferulic acid

senkyunolide I

senkyunolide H

coniferyl ferulate

senkyunolide A

ligustulide and butylidenephthalide) co-existed in the two extracts

with good linear relationship

accuracy

recovery rate

repeatability and stability. As to SFE-CO2 extract of Chuanxiong Rhizoma

their linear range was 2.41-24.14

3.83-38.26

0.81-8.08

47.43-474.32

95.49-954.91

164.91-1 649.14

and 3.32-33.24 ng respectively for the above 7 components

with an average recovery rate of 95.04%

98.24%

99.03%

98.46%

98.13%

96.97%and 95.20% respectively

and RSD of 2.9%

1.2%

1.6%

1.2%

1.1%

1.4% and 1.2%. As to SFE-CO2 extract of Angelicae Sinensis Radix

their linear range was 1.31-13.15

1.70-17.01

0.44-4.43

27.52-275.18

6.46-64.60

206.19-2 061.92 and 3.07-30.65 ng respectively for the above 7 components

with an average recovery rate of 99.03%

99.00%

103.15%

101.78%

102.12%

100.01% and 102.49% respectively

and RSD of 2.1%

2.2%

2.1%

2.5% and 2.2%. Conclusion: Coniferyl ferulate was easily decomposed into ferulic acid. The selection of acetonitrile as solvent for the two extracts can ensure the accurate content determination of original ferulic acid and coniferyl ferulate. The method is simple and rapid

which could provide references for the quality standard for the SFE-CO2 extract from Chuanxiong Rhizoma and Angelicae Sinensis Radix.

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